# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Long, Jeffrey' _publ_contact_author_name 'Dr Jeffrey Long' _publ_contact_author_email jrlong@berkeley.edu _publ_section_title ; Influence of Structure on Exchange Strength and Relaxation Barrier in a Series of FeRe(CN)2 Single-Chain Magnets ; # Attachment '- Structures.cif' # Influence of Structure on Exchange Strength and # Xiaowen Feng, T. David Harris and Jeffrey R. Long* data_xwf3a _database_code_depnum_ccdc_archive 'CCDC 820653' #TrackingRef '- Structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common xwf3a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H20 Cl2 Fe0.50 N3 O2 Re0.50' _chemical_formula_weight 418.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.623 _cell_length_b 10.307 _cell_length_c 10.493 _cell_angle_alpha 104.88 _cell_angle_beta 92.70 _cell_angle_gamma 101.67 _cell_volume 877.9 _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4996 _cell_measurement_theta_min 4.38 _cell_measurement_theta_max 67.73 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 415 _exptl_absorpt_coefficient_mu 4.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7869 _exptl_absorpt_correction_T_max 0.8501 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 7439 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.46 _reflns_number_total 3076 _reflns_number_gt 3045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+1.0973P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3076 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2145(4) 0.0394(4) 0.3581(4) 0.0273(8) Uani 1 1 d . . . C2 C 0.5533(4) 0.0311(3) 0.2059(3) 0.0200(7) Uani 1 1 d . . . C3 C 0.4388(5) -0.2739(4) 0.3030(4) 0.0323(9) Uani 1 1 d . . . C4 C -0.0574(5) -0.0934(5) 0.3307(4) 0.0333(9) Uani 1 1 d . . . H4A H -0.1605 -0.0657 0.3419 0.040 Uiso 1 1 calc R . . H4B H -0.0254 -0.1188 0.4112 0.040 Uiso 1 1 calc R . . C5 C -0.0388(6) 0.2350(5) 0.3456(5) 0.0465(11) Uani 1 1 d . . . H5A H -0.0719 0.2965 0.2976 0.070 Uiso 1 1 calc R . . H5B H 0.0504 0.2869 0.4126 0.070 Uiso 1 1 calc R . . H5C H -0.1283 0.1970 0.3892 0.070 Uiso 1 1 calc R . . C6 C 0.4538(6) -0.5014(4) 0.3251(4) 0.0383(10) Uani 1 1 d . . . H6A H 0.3734 -0.5894 0.2974 0.046 Uiso 1 1 calc R . . H6B H 0.4479 -0.4596 0.4204 0.046 Uiso 1 1 calc R . . C7 C -0.0774(6) -0.2164(5) 0.2116(5) 0.0471(11) Uani 1 1 d . . . H7A H -0.1582 -0.2925 0.2244 0.071 Uiso 1 1 calc R . . H7B H 0.0242 -0.2447 0.2011 0.071 Uiso 1 1 calc R . . H7C H -0.1110 -0.1920 0.1320 0.071 Uiso 1 1 calc R . . C9 C 0.6161(7) -0.5304(6) 0.3071(5) 0.0515(12) Uani 1 1 d . . . H9A H 0.6353 -0.5930 0.3593 0.077 Uiso 1 1 calc R . . H9B H 0.6967 -0.4440 0.3371 0.077 Uiso 1 1 calc R . . H9C H 0.6224 -0.5731 0.2132 0.077 Uiso 1 1 calc R . . C10 C 0.0125(5) 0.1190(5) 0.2494(5) 0.0401(10) Uani 1 1 d . . . H10A H -0.0771 0.0683 0.1807 0.048 Uiso 1 1 calc R . . H10B H 0.1017 0.1579 0.2046 0.048 Uiso 1 1 calc R . . C11 C 0.3316(9) -0.4697(5) 0.1153(5) 0.0599(17) Uani 1 1 d . . . H11A H 0.3415 -0.3977 0.0675 0.072 Uiso 1 1 calc R . . H11B H 0.3841 -0.5418 0.0668 0.072 Uiso 1 1 calc R . . C13 C 0.1605(9) -0.5312(6) 0.1150(8) 0.090(3) Uani 1 1 d . . . H13A H 0.1117 -0.5711 0.0234 0.135 Uiso 1 1 calc R . . H13B H 0.1069 -0.4597 0.1603 0.135 Uiso 1 1 calc R . . H13C H 0.1498 -0.6034 0.1613 0.135 Uiso 1 1 calc R . . N1 N 0.5698(3) 0.0408(3) 0.3174(3) 0.0235(6) Uani 1 1 d . . . N2 N 0.0630(4) 0.0227(4) 0.3155(3) 0.0290(7) Uani 1 1 d . . . N3 N 0.4142(5) -0.4088(3) 0.2491(3) 0.0349(8) Uani 1 1 d . . . O1 O 0.2641(3) -0.0382(3) 0.4169(2) 0.0251(5) Uani 1 1 d . . . O2 O 0.5000(3) -0.2139(3) 0.4182(2) 0.0293(6) Uani 1 1 d . . . Cl1 Cl 0.26574(10) -0.15708(9) 0.00761(9) 0.0285(2) Uani 1 1 d . . . Cl2 Cl 0.63659(12) -0.17785(9) -0.04347(9) 0.0312(2) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 0.5000 0.02457(17) Uani 1 2 d S . . Re1 Re 0.5000 0.0000 0.0000 0.02240(9) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0214(18) 0.043(2) 0.0199(16) 0.0066(15) 0.0043(14) 0.0139(16) C2 0.0151(15) 0.0249(16) 0.0221(18) 0.0075(13) 0.0028(13) 0.0073(13) C3 0.045(2) 0.0307(19) 0.0227(18) 0.0081(15) 0.0031(17) 0.0119(17) C4 0.0204(18) 0.051(2) 0.0287(19) 0.0099(18) 0.0023(15) 0.0098(17) C5 0.033(2) 0.052(3) 0.058(3) 0.018(2) -0.003(2) 0.015(2) C6 0.057(3) 0.036(2) 0.0278(19) 0.0142(17) 0.0030(19) 0.019(2) C7 0.043(3) 0.055(3) 0.040(2) 0.009(2) 0.001(2) 0.012(2) C9 0.057(3) 0.058(3) 0.043(3) 0.012(2) 0.001(2) 0.024(3) C10 0.028(2) 0.063(3) 0.039(2) 0.025(2) 0.0018(18) 0.019(2) C11 0.124(5) 0.028(2) 0.027(2) 0.0040(18) -0.016(3) 0.024(3) C13 0.099(5) 0.050(3) 0.100(5) -0.024(3) -0.063(4) 0.042(4) N1 0.0183(14) 0.0326(16) 0.0202(16) 0.0078(12) 0.0023(11) 0.0066(12) N2 0.0199(15) 0.049(2) 0.0226(15) 0.0133(14) 0.0021(12) 0.0131(14) N3 0.058(2) 0.0269(16) 0.0222(16) 0.0090(13) -0.0020(15) 0.0135(16) O1 0.0187(12) 0.0402(14) 0.0184(12) 0.0094(10) 0.0003(9) 0.0098(11) O2 0.0367(15) 0.0337(14) 0.0179(12) 0.0037(10) -0.0018(11) 0.0141(12) Cl1 0.0241(4) 0.0361(5) 0.0258(4) 0.0163(4) -0.0020(3) -0.0015(4) Cl2 0.0387(5) 0.0315(5) 0.0299(5) 0.0083(4) 0.0052(4) 0.0220(4) Fe1 0.0212(4) 0.0363(4) 0.0171(3) 0.0063(3) 0.0004(3) 0.0101(3) Re1 0.02478(13) 0.02581(12) 0.01872(12) 0.00768(8) 0.00244(8) 0.00828(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.253(5) . ? C1 N2 1.323(5) . ? C2 N1 1.148(5) . ? C2 Re1 2.115(3) . ? C3 O2 1.243(5) . ? C3 N3 1.328(5) . ? C4 N2 1.465(5) . ? C4 C7 1.508(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.511(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N3 1.470(5) . ? C6 C9 1.500(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N2 1.468(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C13 1.483(10) . ? C11 N3 1.465(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? N1 Fe1 2.152(3) . ? O1 Fe1 2.094(2) . ? O2 Fe1 2.151(3) . ? Cl1 Re1 2.3382(8) . ? Cl2 Re1 2.3345(9) . ? Fe1 O1 2.094(2) 2_656 ? Fe1 O2 2.151(3) 2_656 ? Fe1 N1 2.152(3) 2_656 ? Re1 C2 2.115(3) 2_655 ? Re1 Cl2 2.3345(9) 2_655 ? Re1 Cl1 2.3382(8) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N2 123.3(4) . . ? N1 C2 Re1 174.2(3) . . ? O2 C3 N3 124.4(4) . . ? N2 C4 C7 111.1(4) . . ? N2 C4 H4A 109.4 . . ? C7 C4 H4A 109.4 . . ? N2 C4 H4B 109.4 . . ? C7 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C10 C5 H5A 109.5 . . ? C10 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C10 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C9 113.2(4) . . ? N3 C6 H6A 108.9 . . ? C9 C6 H6A 108.9 . . ? N3 C6 H6B 108.9 . . ? C9 C6 H6B 108.9 . . ? H6A C6 H6B 107.8 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C5 112.1(4) . . ? N2 C10 H10A 109.2 . . ? C5 C10 H10A 109.2 . . ? N2 C10 H10B 109.2 . . ? C5 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C13 C11 N3 113.0(5) . . ? C13 C11 H11A 109.0 . . ? N3 C11 H11A 109.0 . . ? C13 C11 H11B 109.0 . . ? N3 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 N1 Fe1 154.8(3) . . ? C1 N2 C4 120.9(3) . . ? C1 N2 C10 120.5(3) . . ? C4 N2 C10 118.5(3) . . ? C3 N3 C11 119.7(3) . . ? C3 N3 C6 121.6(3) . . ? C11 N3 C6 118.4(3) . . ? C1 O1 Fe1 123.0(2) . . ? C3 O2 Fe1 119.7(2) . . ? O1 Fe1 O1 180.0 2_656 . ? O1 Fe1 O2 89.39(10) 2_656 2_656 ? O1 Fe1 O2 90.61(10) . 2_656 ? O1 Fe1 O2 90.61(10) 2_656 . ? O1 Fe1 O2 89.39(10) . . ? O2 Fe1 O2 180.0 2_656 . ? O1 Fe1 N1 86.91(10) 2_656 2_656 ? O1 Fe1 N1 93.09(10) . 2_656 ? O2 Fe1 N1 89.75(11) 2_656 2_656 ? O2 Fe1 N1 90.25(11) . 2_656 ? O1 Fe1 N1 93.09(10) 2_656 . ? O1 Fe1 N1 86.91(10) . . ? O2 Fe1 N1 90.25(11) 2_656 . ? O2 Fe1 N1 89.75(11) . . ? N1 Fe1 N1 180.0 2_656 . ? C2 Re1 C2 180.00(18) 2_655 . ? C2 Re1 Cl2 89.91(9) 2_655 2_655 ? C2 Re1 Cl2 90.09(9) . 2_655 ? C2 Re1 Cl2 90.09(9) 2_655 . ? C2 Re1 Cl2 89.91(9) . . ? Cl2 Re1 Cl2 180.00(6) 2_655 . ? C2 Re1 Cl1 91.18(9) 2_655 . ? C2 Re1 Cl1 88.82(9) . . ? Cl2 Re1 Cl1 89.89(3) 2_655 . ? Cl2 Re1 Cl1 90.11(3) . . ? C2 Re1 Cl1 88.82(9) 2_655 2_655 ? C2 Re1 Cl1 91.18(9) . 2_655 ? Cl2 Re1 Cl1 90.11(3) 2_655 2_655 ? Cl2 Re1 Cl1 89.89(3) . 2_655 ? Cl1 Re1 Cl1 180.00(6) . 2_655 ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.074 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.118 #===END data_xwf9a _database_code_depnum_ccdc_archive 'CCDC 820654' #TrackingRef '- Structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common xwf9a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H72 Cl4 Fe N6 O4 Re' _chemical_formula_weight 1060.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9348(6) _cell_length_b 10.5040(7) _cell_length_c 14.0627(10) _cell_angle_alpha 68.984(4) _cell_angle_beta 77.296(4) _cell_angle_gamma 85.408(4) _cell_volume 1201.85(14) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6615 _cell_measurement_theta_min 3.44 _cell_measurement_theta_max 65.25 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 543 _exptl_absorpt_coefficient_mu 9.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5954 _exptl_absorpt_correction_T_max 0.6990 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'microfocus rotating anode' _diffrn_radiation_monochromator 'HELIOS multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 8853 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 65.25 _reflns_number_total 3947 _reflns_number_gt 3698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+2.4100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3947 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7936(7) 0.3423(6) 0.4923(5) 0.0328(13) Uani 1 1 d . . . C2 C 0.4580(6) 0.2076(6) 0.4824(5) 0.0295(12) Uani 1 1 d . . . C3 C 1.0007(7) 0.2100(7) 0.6820(5) 0.0375(14) Uani 1 1 d . . . H3A H 1.0583 0.1358 0.6621 0.045 Uiso 1 1 calc R . . H3B H 1.0563 0.2338 0.7269 0.045 Uiso 1 1 calc R . . C4 C 0.9983(7) 0.3350(7) 0.5833(5) 0.0377(14) Uani 1 1 d . . . H4A H 0.9363 0.4079 0.6024 0.045 Uiso 1 1 calc R . . H4B H 1.1043 0.3696 0.5516 0.045 Uiso 1 1 calc R . . C5 C 1.0324(7) 0.2362(7) 0.4402(6) 0.0414(15) Uani 1 1 d . . . H5A H 0.9671 0.1911 0.4131 0.050 Uiso 1 1 calc R . . H5B H 1.0939 0.1648 0.4828 0.050 Uiso 1 1 calc R . . C6 C 1.1399(8) 0.3357(8) 0.3491(6) 0.0439(16) Uani 1 1 d . . . H6A H 1.2188 0.2826 0.3176 0.053 Uiso 1 1 calc R . . H6B H 1.1933 0.3900 0.3762 0.053 Uiso 1 1 calc R . . C7 C 0.8419(7) 0.1576(7) 0.7445(5) 0.0404(14) Uani 1 1 d . . . H7A H 0.7930 0.2221 0.7789 0.049 Uiso 1 1 calc R . . H7B H 0.7775 0.1534 0.6966 0.049 Uiso 1 1 calc R . . C8 C 0.7392(7) 0.9983(7) 0.1090(5) 0.0382(14) Uani 1 1 d . . . H8A H 0.7683 0.9927 0.1744 0.046 Uiso 1 1 calc R . . H8B H 0.8277 0.9668 0.0668 0.046 Uiso 1 1 calc R . . C9 C 0.5857(7) 0.7068(7) 0.2902(5) 0.0356(13) Uani 1 1 d . . . C10 C 0.6025(7) 0.9056(7) 0.1346(5) 0.0387(14) Uani 1 1 d . . . H10A H 0.5158 0.9355 0.1792 0.046 Uiso 1 1 calc R . . H10B H 0.5704 0.9157 0.0692 0.046 Uiso 1 1 calc R . . C11 C 0.7258(7) 0.6845(7) 0.1276(6) 0.0427(15) Uani 1 1 d . . . H11A H 0.7663 0.6017 0.1758 0.051 Uiso 1 1 calc R . . H11B H 0.8145 0.7405 0.0801 0.051 Uiso 1 1 calc R . . C12 C 0.6353(9) 0.6421(9) 0.0637(6) 0.0545(19) Uani 1 1 d . . . H12A H 0.7062 0.5990 0.0193 0.065 Uiso 1 1 calc R . . H12B H 0.5920 0.7247 0.0173 0.065 Uiso 1 1 calc R . . C14 C 0.7027(8) 1.1448(7) 0.0498(6) 0.0407(15) Uani 1 1 d . . . H14A H 0.6194 1.1781 0.0943 0.049 Uiso 1 1 calc R . . H14B H 0.6655 1.1489 -0.0126 0.049 Uiso 1 1 calc R . . C15 C 1.0628(8) 0.4344(8) 0.2630(6) 0.0467(16) Uani 1 1 d . . . H15A H 0.9709 0.4744 0.2958 0.056 Uiso 1 1 calc R . . H15B H 1.1347 0.5098 0.2187 0.056 Uiso 1 1 calc R . . C16 C 0.8492(9) 0.0168(8) 0.8264(6) 0.0516(18) Uani 1 1 d . . . H16A H 0.8999 -0.0468 0.7927 0.077 Uiso 1 1 calc R . . H16B H 0.7449 -0.0152 0.8629 0.077 Uiso 1 1 calc R . . H16C H 0.9074 0.0218 0.8765 0.077 Uiso 1 1 calc R . . C18 C 1.0154(10) 0.3685(9) 0.1951(6) 0.0540(18) Uani 1 1 d . . . H18A H 1.1046 0.3245 0.1651 0.081 Uiso 1 1 calc R . . H18B H 0.9746 0.4382 0.1390 0.081 Uiso 1 1 calc R . . H18C H 0.9361 0.3001 0.2370 0.081 Uiso 1 1 calc R . . C19 C 0.8407(9) 1.2372(8) 0.0162(7) 0.0544(19) Uani 1 1 d . . . H19A H 0.8878 1.2226 0.0760 0.082 Uiso 1 1 calc R . . H19B H 0.8081 1.3325 -0.0104 0.082 Uiso 1 1 calc R . . H19C H 0.9155 1.2162 -0.0386 0.082 Uiso 1 1 calc R . . C20 C 0.5049(9) 0.5429(11) 0.1302(8) 0.067(2) Uani 1 1 d . . . H20A H 0.4382 0.5830 0.1784 0.080 Uiso 1 1 calc R . . H20B H 0.4420 0.5309 0.0841 0.080 Uiso 1 1 calc R . . C21 C 0.5592(11) 0.4067(10) 0.1918(8) 0.073(3) Uani 1 1 d . . . H21A H 0.6275 0.3673 0.1448 0.109 Uiso 1 1 calc R . . H21B H 0.4708 0.3465 0.2297 0.109 Uiso 1 1 calc R . . H21C H 0.6149 0.4168 0.2414 0.109 Uiso 1 1 calc R . . N1 N 0.9342(6) 0.3035(5) 0.5060(4) 0.0340(11) Uani 1 1 d . . . N2 N 0.4482(6) 0.3187(5) 0.4771(4) 0.0330(11) Uani 1 1 d . . . N3 N 0.6342(6) 0.7619(6) 0.1876(4) 0.0381(12) Uani 1 1 d . . . O1 O 0.6117(5) 0.5880(4) 0.3422(3) 0.0367(10) Uani 1 1 d . . . O2 O 0.7061(4) 0.4081(4) 0.5408(3) 0.0310(9) Uani 1 1 d . . . Cl1 Cl 0.72160(18) 0.06450(17) 0.37045(14) 0.0466(4) Uani 1 1 d . . . Cl2 Cl 0.6379(2) -0.01421(17) 0.62632(15) 0.0476(4) Uani 1 1 d . . . Fe1 Fe 0.5000 0.5000 0.5000 0.0267(3) Uani 1 2 d S . . Re1 Re 0.5000 0.0000 0.5000 0.03185(17) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(3) 0.026(3) 0.043(3) -0.007(3) -0.011(2) 0.000(2) C2 0.027(3) 0.021(3) 0.041(3) -0.008(2) -0.013(2) 0.001(2) C3 0.032(3) 0.034(3) 0.048(4) -0.012(3) -0.017(3) 0.006(2) C4 0.033(3) 0.034(3) 0.046(3) -0.012(3) -0.013(3) 0.004(2) C5 0.033(3) 0.039(4) 0.056(4) -0.021(3) -0.015(3) 0.011(3) C6 0.033(3) 0.049(4) 0.049(4) -0.019(3) -0.008(3) 0.011(3) C7 0.035(3) 0.043(4) 0.045(3) -0.013(3) -0.015(3) 0.001(3) C8 0.037(3) 0.038(4) 0.037(3) -0.008(3) -0.011(3) 0.002(3) C9 0.029(3) 0.034(3) 0.045(3) -0.014(3) -0.010(3) -0.001(2) C10 0.033(3) 0.039(4) 0.040(3) -0.007(3) -0.010(3) 0.001(3) C11 0.032(3) 0.038(4) 0.049(4) -0.009(3) -0.001(3) 0.002(3) C12 0.053(4) 0.060(5) 0.054(4) -0.024(4) -0.016(4) 0.012(4) C14 0.039(3) 0.035(4) 0.049(4) -0.015(3) -0.011(3) 0.000(3) C15 0.036(3) 0.048(4) 0.054(4) -0.014(3) -0.013(3) 0.003(3) C16 0.046(4) 0.051(5) 0.051(4) -0.007(3) -0.014(3) -0.004(3) C18 0.057(4) 0.054(5) 0.054(4) -0.019(4) -0.016(4) 0.003(4) C19 0.043(4) 0.047(4) 0.068(5) -0.014(4) -0.009(3) -0.008(3) C20 0.043(4) 0.089(7) 0.088(6) -0.057(6) -0.007(4) -0.002(4) C21 0.067(6) 0.067(6) 0.080(6) -0.037(5) 0.018(5) -0.025(5) N1 0.029(2) 0.031(3) 0.041(3) -0.012(2) -0.010(2) 0.004(2) N2 0.030(2) 0.024(3) 0.044(3) -0.009(2) -0.012(2) 0.0035(19) N3 0.029(2) 0.037(3) 0.043(3) -0.008(2) -0.008(2) 0.000(2) O1 0.036(2) 0.030(2) 0.040(2) -0.0077(19) -0.0068(18) 0.0038(17) O2 0.0263(19) 0.026(2) 0.042(2) -0.0129(18) -0.0104(17) 0.0039(15) Cl1 0.0390(8) 0.0356(9) 0.0643(10) -0.0202(8) -0.0051(7) 0.0020(6) Cl2 0.0514(9) 0.0381(9) 0.0663(10) -0.0238(8) -0.0338(8) 0.0133(7) Fe1 0.0247(6) 0.0188(6) 0.0371(7) -0.0093(5) -0.0091(5) 0.0025(5) Re1 0.0311(2) 0.0217(2) 0.0478(3) -0.01522(17) -0.01425(16) 0.00340(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.253(7) . ? C1 N1 1.323(8) . ? C2 N2 1.140(8) . ? C2 Re1 2.116(6) . ? C3 C7 1.522(9) . ? C3 C4 1.534(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.476(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.462(9) . ? C5 C6 1.522(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C15 1.538(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C16 1.521(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C14 1.513(9) . ? C8 C10 1.522(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O1 1.232(8) . ? C9 N3 1.331(9) . ? C10 N3 1.461(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N3 1.458(9) . ? C11 C12 1.524(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C20 1.528(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C19 1.513(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C18 1.506(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.489(15) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N2 Fe1 2.143(5) . ? O1 Fe1 2.116(4) . ? O2 Fe1 2.106(4) . ? Cl1 Re1 2.3326(16) . ? Cl2 Re1 2.3322(16) . ? Fe1 O2 2.106(4) 2_666 ? Fe1 O1 2.116(4) 2_666 ? Fe1 N2 2.143(5) 2_666 ? Re1 C2 2.116(6) 2_656 ? Re1 Cl2 2.3322(16) 2_656 ? Re1 Cl1 2.3326(16) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 N1 124.3(6) . . ? N2 C2 Re1 173.1(5) . . ? C7 C3 C4 113.8(5) . . ? C7 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? C7 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N1 C4 C3 112.3(5) . . ? N1 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N1 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C6 112.3(6) . . ? N1 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C15 115.4(6) . . ? C5 C6 H6A 108.4 . . ? C15 C6 H6A 108.4 . . ? C5 C6 H6B 108.4 . . ? C15 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C16 C7 C3 111.8(6) . . ? C16 C7 H7A 109.3 . . ? C3 C7 H7A 109.3 . . ? C16 C7 H7B 109.3 . . ? C3 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C14 C8 C10 111.3(5) . . ? C14 C8 H8A 109.4 . . ? C10 C8 H8A 109.4 . . ? C14 C8 H8B 109.4 . . ? C10 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? O1 C9 N3 123.9(6) . . ? N3 C10 C8 113.4(5) . . ? N3 C10 H10A 108.9 . . ? C8 C10 H10A 108.9 . . ? N3 C10 H10B 108.9 . . ? C8 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N3 C11 C12 113.0(6) . . ? N3 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N3 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C20 113.5(7) . . ? C11 C12 H12A 108.9 . . ? C20 C12 H12A 108.9 . . ? C11 C12 H12B 108.9 . . ? C20 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C8 C14 C19 112.3(6) . . ? C8 C14 H14A 109.1 . . ? C19 C14 H14A 109.1 . . ? C8 C14 H14B 109.1 . . ? C19 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C18 C15 C6 113.8(7) . . ? C18 C15 H15A 108.8 . . ? C6 C15 H15A 108.8 . . ? C18 C15 H15B 108.8 . . ? C6 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C7 C16 H16A 109.5 . . ? C7 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C7 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C12 113.4(7) . . ? C21 C20 H20A 108.9 . . ? C12 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? C12 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C1 N1 C5 120.4(5) . . ? C1 N1 C4 120.7(5) . . ? C5 N1 C4 118.8(5) . . ? C2 N2 Fe1 157.6(5) . . ? C9 N3 C11 121.6(6) . . ? C9 N3 C10 119.2(6) . . ? C11 N3 C10 119.0(5) . . ? C9 O1 Fe1 121.0(4) . . ? C1 O2 Fe1 123.9(4) . . ? O2 Fe1 O2 180.0(2) 2_666 . ? O2 Fe1 O1 91.06(16) 2_666 2_666 ? O2 Fe1 O1 88.94(16) . 2_666 ? O2 Fe1 O1 88.94(16) 2_666 . ? O2 Fe1 O1 91.06(16) . . ? O1 Fe1 O1 180.000(1) 2_666 . ? O2 Fe1 N2 91.13(17) 2_666 . ? O2 Fe1 N2 88.87(17) . . ? O1 Fe1 N2 88.36(18) 2_666 . ? O1 Fe1 N2 91.64(18) . . ? O2 Fe1 N2 88.87(17) 2_666 2_666 ? O2 Fe1 N2 91.13(17) . 2_666 ? O1 Fe1 N2 91.64(18) 2_666 2_666 ? O1 Fe1 N2 88.36(18) . 2_666 ? N2 Fe1 N2 180.0(3) . 2_666 ? C2 Re1 C2 180.000(1) 2_656 . ? C2 Re1 Cl2 87.89(16) 2_656 2_656 ? C2 Re1 Cl2 92.11(16) . 2_656 ? C2 Re1 Cl2 92.11(16) 2_656 . ? C2 Re1 Cl2 87.89(16) . . ? Cl2 Re1 Cl2 180.0 2_656 . ? C2 Re1 Cl1 90.79(16) 2_656 . ? C2 Re1 Cl1 89.21(16) . . ? Cl2 Re1 Cl1 89.52(7) 2_656 . ? Cl2 Re1 Cl1 90.48(7) . . ? C2 Re1 Cl1 89.21(16) 2_656 2_656 ? C2 Re1 Cl1 90.79(16) . 2_656 ? Cl2 Re1 Cl1 90.48(7) 2_656 2_656 ? Cl2 Re1 Cl1 89.52(7) . 2_656 ? Cl1 Re1 Cl1 180.0 . 2_656 ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 65.25 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 3.693 _refine_diff_density_min -0.876 _refine_diff_density_rms 0.186 #===END data_xwf22a _database_code_depnum_ccdc_archive 'CCDC 820655' #TrackingRef '- Structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common xwf22a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H26 Cl2 Fe0.50 N3 O2 Re0.50' _chemical_formula_weight 448.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.778 _cell_length_b 12.316 _cell_length_c 14.407 _cell_angle_alpha 90.00 _cell_angle_beta 107.01 _cell_angle_gamma 90.00 _cell_volume 1828.7 _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 7812 _cell_measurement_theta_min 4.54 _cell_measurement_theta_max 67.88 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 4.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7655 _exptl_absorpt_correction_T_max 0.8238 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 14876 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.42 _reflns_number_total 3193 _reflns_number_gt 2540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+13.6758P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3193 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C9 C 0.0721(9) -0.1564(8) 0.3504(8) 0.052(2) Uani 1 1 d . . . C12 C 0.0756(7) -0.1738(7) 0.6735(6) 0.0381(19) Uani 1 1 d . . . C14 C 0.1679(12) -0.3066(10) 0.4519(11) 0.084(4) Uani 1 1 d . . . H14A H 0.1886 -0.2588 0.5088 0.127 Uiso 1 1 calc R . . H14B H 0.2397 -0.3574 0.4575 0.127 Uiso 1 1 calc R . . H14C H 0.0885 -0.3473 0.4483 0.127 Uiso 1 1 calc R . . C50 C 0.2224(9) -0.2734(9) 0.2996(9) 0.067(3) Uani 1 1 d . . . H50A H 0.1858 -0.2380 0.2366 0.100 Uiso 1 1 calc R . . H50B H 0.2183 -0.3524 0.2910 0.100 Uiso 1 1 calc R . . H50C H 0.3131 -0.2511 0.3271 0.100 Uiso 1 1 calc R . . C51 C 0.0708(11) -0.0727(12) 0.2653(11) 0.092(5) Uani 1 1 d . . . H51A H 0.0824 0.0024 0.2911 0.111 Uiso 1 1 calc R . . H51B H 0.1426 -0.0893 0.2377 0.111 Uiso 1 1 calc R . . C52 C -0.045(2) -0.0817(16) 0.1953(16) 0.149(9) Uani 1 1 d . . . H52A H -0.1179 -0.0656 0.2222 0.178 Uiso 1 1 calc R . . H52B H -0.0568 -0.1559 0.1676 0.178 Uiso 1 1 calc R . . C53 C -0.040(3) 0.0051(13) 0.1148(13) 0.160(12) Uani 1 1 d . . . H53A H -0.0279 0.0778 0.1437 0.241 Uiso 1 1 calc R . . H53B H -0.1210 0.0028 0.0618 0.241 Uiso 1 1 calc R . . H53C H 0.0331 -0.0118 0.0895 0.241 Uiso 1 1 calc R . . C56 C 0.3019(8) -0.1404(9) 0.7522(8) 0.060(3) Uani 1 1 d . . . H56A H 0.3155 -0.1327 0.6882 0.090 Uiso 1 1 calc R . . H56B H 0.3758 -0.1788 0.7958 0.090 Uiso 1 1 calc R . . H56C H 0.2940 -0.0684 0.7787 0.090 Uiso 1 1 calc R . . C60 C -0.0500(8) -0.2343(7) 0.6642(7) 0.042(2) Uani 1 1 d . . . H60A H -0.1227 -0.1818 0.6503 0.050 Uiso 1 1 calc R . . H60B H -0.0449 -0.2705 0.7265 0.050 Uiso 1 1 calc R . . C61 C -0.0769(12) -0.3196(10) 0.5829(8) 0.070(3) Uani 1 1 d . . . H61A H -0.0777 -0.2831 0.5215 0.084 Uiso 1 1 calc R . . H61B H -0.0048 -0.3727 0.5984 0.084 Uiso 1 1 calc R . . C63 C 0.1890(8) -0.2865(8) 0.8153(7) 0.051(2) Uani 1 1 d . . . H63A H 0.1591 -0.2569 0.8681 0.076 Uiso 1 1 calc R . . H63B H 0.2789 -0.3114 0.8412 0.076 Uiso 1 1 calc R . . H63C H 0.1337 -0.3478 0.7853 0.076 Uiso 1 1 calc R . . C66 C -0.1946(16) -0.3763(14) 0.5684(12) 0.108(5) Uani 1 1 d . . . H66A H -0.1924 -0.4172 0.6272 0.162 Uiso 1 1 calc R . . H66B H -0.2066 -0.4265 0.5137 0.162 Uiso 1 1 calc R . . H66C H -0.2668 -0.3245 0.5542 0.162 Uiso 1 1 calc R . . C100 C 0.3043(7) 0.0186(6) 0.4999(6) 0.0277(16) Uani 1 1 d . . . N1 N 0.1991(6) 0.0287(6) 0.5004(5) 0.0336(15) Uani 1 1 d . . . N12 N 0.1485(7) -0.2419(6) 0.3651(6) 0.052(2) Uani 1 1 d . . . N15 N 0.1820(6) -0.2028(6) 0.7429(5) 0.0411(17) Uani 1 1 d . . . O2 O 0.0803(5) -0.0987(5) 0.6177(5) 0.0468(16) Uani 1 1 d . . . O11 O 0.0045(5) -0.1356(5) 0.4061(5) 0.0477(16) Uani 1 1 d . . . Cl1 Cl 0.56535(18) 0.01778(16) 0.66890(15) 0.0356(4) Uani 1 1 d . . . Cl2 Cl 0.51175(19) 0.18822(16) 0.48382(16) 0.0427(5) Uani 1 1 d . . . Fe1 Fe 0.0000 0.0000 0.5000 0.0299(4) Uani 1 2 d S . . Re1 Re 0.5000 0.0000 0.5000 0.03153(19) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C9 0.046(5) 0.061(6) 0.052(6) -0.020(5) 0.021(5) -0.021(5) C12 0.027(4) 0.044(4) 0.050(5) 0.002(4) 0.020(4) 0.009(3) C14 0.074(8) 0.068(8) 0.130(12) 0.030(8) 0.061(8) 0.017(6) C50 0.042(5) 0.080(7) 0.085(8) -0.039(6) 0.030(5) -0.007(5) C51 0.042(6) 0.109(11) 0.128(12) -0.069(10) 0.029(7) -0.005(6) C52 0.17(2) 0.128(16) 0.159(19) -0.096(15) 0.064(16) -0.072(14) C53 0.31(4) 0.096(14) 0.064(11) -0.006(9) 0.040(16) -0.015(15) C56 0.024(4) 0.064(6) 0.084(8) 0.026(6) 0.002(4) -0.011(4) C60 0.038(5) 0.046(5) 0.043(5) 0.008(4) 0.015(4) 0.003(4) C61 0.077(8) 0.084(8) 0.062(7) 0.004(6) 0.038(6) -0.029(6) C63 0.035(5) 0.064(6) 0.050(6) 0.020(5) 0.007(4) 0.002(4) C66 0.116(13) 0.116(12) 0.089(11) 0.018(10) 0.026(10) 0.000(10) C100 0.019(4) 0.033(4) 0.030(4) -0.003(3) 0.006(3) 0.003(3) N1 0.024(4) 0.042(4) 0.033(4) -0.001(3) 0.006(3) 0.000(3) N12 0.030(4) 0.050(4) 0.079(6) -0.030(4) 0.020(4) 0.000(3) N15 0.028(3) 0.050(4) 0.043(4) 0.018(3) 0.007(3) 0.004(3) O2 0.028(3) 0.059(4) 0.053(4) 0.033(3) 0.011(3) 0.010(3) O11 0.032(3) 0.046(3) 0.071(5) -0.022(3) 0.026(3) -0.009(3) Cl1 0.0252(9) 0.0445(10) 0.0356(11) -0.0027(8) 0.0064(8) 0.0024(7) Cl2 0.0395(11) 0.0283(10) 0.0581(14) 0.0006(9) 0.0106(10) -0.0036(8) Fe1 0.0202(7) 0.0338(8) 0.0354(9) 0.0013(7) 0.0076(6) 0.0027(6) Re1 0.0205(2) 0.0322(3) 0.0419(3) 0.0004(2) 0.00918(18) 0.00043(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C9 O11 1.258(11) . ? C9 N12 1.316(13) . ? C9 C51 1.599(19) . ? C12 O2 1.235(10) . ? C12 N15 1.331(10) . ? C12 C60 1.516(11) . ? C14 N12 1.445(15) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C50 N12 1.454(12) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.36(2) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.59(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C56 N15 1.475(10) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C60 C61 1.536(14) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C66 1.409(19) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C63 N15 1.452(11) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C100 N1 1.142(11) . ? C100 Re1 2.122(7) . ? N1 Fe1 2.174(7) . ? O2 Fe1 2.060(5) . ? O11 Fe1 2.158(6) . ? Cl1 Re1 2.337(2) . ? Cl2 Re1 2.337(2) . ? Fe1 O2 2.060(5) 3_556 ? Fe1 O11 2.158(6) 3_556 ? Fe1 N1 2.174(7) 3_556 ? Re1 C100 2.122(7) 3_656 ? Re1 Cl2 2.337(2) 3_656 ? Re1 Cl1 2.337(2) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 C9 N12 120.8(10) . . ? O11 C9 C51 118.8(9) . . ? N12 C9 C51 120.3(9) . . ? O2 C12 N15 119.9(7) . . ? O2 C12 C60 121.0(7) . . ? N15 C12 C60 119.0(7) . . ? N12 C14 H14A 109.5 . . ? N12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N12 C50 H50A 109.5 . . ? N12 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N12 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C9 108.4(14) . . ? C52 C51 H51A 110.0 . . ? C9 C51 H51A 110.0 . . ? C52 C51 H51B 110.0 . . ? C9 C51 H51B 110.0 . . ? H51A C51 H51B 108.4 . . ? C51 C52 C53 105.2(17) . . ? C51 C52 H52A 110.7 . . ? C53 C52 H52A 110.7 . . ? C51 C52 H52B 110.7 . . ? C53 C52 H52B 110.7 . . ? H52A C52 H52B 108.8 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N15 C56 H56A 109.5 . . ? N15 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N15 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C12 C60 C61 111.6(7) . . ? C12 C60 H60A 109.3 . . ? C61 C60 H60A 109.3 . . ? C12 C60 H60B 109.3 . . ? C61 C60 H60B 109.3 . . ? H60A C60 H60B 108.0 . . ? C66 C61 C60 114.4(11) . . ? C66 C61 H61A 108.7 . . ? C60 C61 H61A 108.7 . . ? C66 C61 H61B 108.7 . . ? C60 C61 H61B 108.7 . . ? H61A C61 H61B 107.6 . . ? N15 C63 H63A 109.5 . . ? N15 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N15 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N1 C100 Re1 179.7(8) . . ? C100 N1 Fe1 164.4(6) . . ? C9 N12 C14 120.4(9) . . ? C9 N12 C50 123.0(10) . . ? C14 N12 C50 116.5(9) . . ? C12 N15 C63 125.6(7) . . ? C12 N15 C56 117.9(7) . . ? C63 N15 C56 116.4(7) . . ? C12 O2 Fe1 152.8(6) . . ? C9 O11 Fe1 132.9(6) . . ? O2 Fe1 O2 180.000(1) 3_556 . ? O2 Fe1 O11 88.7(3) 3_556 3_556 ? O2 Fe1 O11 91.3(3) . 3_556 ? O2 Fe1 O11 91.3(3) 3_556 . ? O2 Fe1 O11 88.7(3) . . ? O11 Fe1 O11 180.0 3_556 . ? O2 Fe1 N1 85.3(2) 3_556 3_556 ? O2 Fe1 N1 94.7(2) . 3_556 ? O11 Fe1 N1 85.6(2) 3_556 3_556 ? O11 Fe1 N1 94.4(2) . 3_556 ? O2 Fe1 N1 94.7(2) 3_556 . ? O2 Fe1 N1 85.3(2) . . ? O11 Fe1 N1 94.4(2) 3_556 . ? O11 Fe1 N1 85.6(2) . . ? N1 Fe1 N1 180.000(1) 3_556 . ? C100 Re1 C100 180.000(1) 3_656 . ? C100 Re1 Cl2 88.6(2) 3_656 3_656 ? C100 Re1 Cl2 91.4(2) . 3_656 ? C100 Re1 Cl2 91.4(2) 3_656 . ? C100 Re1 Cl2 88.6(2) . . ? Cl2 Re1 Cl2 180.000(13) 3_656 . ? C100 Re1 Cl1 90.7(2) 3_656 . ? C100 Re1 Cl1 89.3(2) . . ? Cl2 Re1 Cl1 89.87(7) 3_656 . ? Cl2 Re1 Cl1 90.13(7) . . ? C100 Re1 Cl1 89.3(2) 3_656 3_656 ? C100 Re1 Cl1 90.7(2) . 3_656 ? Cl2 Re1 Cl1 90.13(7) 3_656 3_656 ? Cl2 Re1 Cl1 89.87(7) . 3_656 ? Cl1 Re1 Cl1 180.0 . 3_656 ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.690 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.176 #===END data_xwf17 _database_code_depnum_ccdc_archive 'CCDC 820656' #TrackingRef '- Structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common xwf-17 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H22 Cl2 Fe0.50 N3 O2 Re0.50' _chemical_formula_weight 420.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.465 _cell_length_b 9.976 _cell_length_c 10.631 _cell_angle_alpha 108.44 _cell_angle_beta 109.42 _cell_angle_gamma 106.27 _cell_volume 810.6 _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 8631 _cell_measurement_theta_min 4.95 _cell_measurement_theta_max 68.25 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 419 _exptl_absorpt_coefficient_mu 4.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7126 _exptl_absorpt_correction_T_max 0.8391 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 8928 _diffrn_reflns_av_R_equivalents 0.0144 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.37 _reflns_number_total 2840 _reflns_number_gt 2821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+3.2140P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2840 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.0736(5) -0.1964(5) 0.1662(5) 0.0141(8) Uani 1 1 d . . . C3 C 0.2016(6) -0.0869(5) 0.3270(5) 0.0196(9) Uani 1 1 d . . . H3A H 0.2905 -0.0030 0.3301 0.024 Uiso 1 1 calc R . . H3B H 0.2524 -0.1456 0.3716 0.024 Uiso 1 1 calc R . . C4 C -0.2563(5) 0.0132(5) 0.1339(5) 0.0176(9) Uani 1 1 d . . . C5 C -0.0996(6) 0.2816(5) 0.3534(5) 0.0239(10) Uani 1 1 d . . . H5A H -0.0693 0.3930 0.3817 0.036 Uiso 1 1 calc R . . H5B H 0.0012 0.2649 0.3824 0.036 Uiso 1 1 calc R . . H5C H -0.1610 0.2481 0.4045 0.036 Uiso 1 1 calc R . . C6 C -0.2082(6) 0.1866(6) 0.1847(5) 0.0223(10) Uani 1 1 d . . . H6A H -0.3099 0.2037 0.1558 0.027 Uiso 1 1 calc R . . H6B H -0.1474 0.2236 0.1335 0.027 Uiso 1 1 calc R . . C7 C -0.1698(6) -0.4360(6) -0.0241(6) 0.0305(11) Uani 1 1 d . . . H7A H -0.2419 -0.5331 -0.0310 0.046 Uiso 1 1 calc R . . H7B H -0.1197 -0.4608 -0.0904 0.046 Uiso 1 1 calc R . . H7C H -0.2356 -0.3810 -0.0543 0.046 Uiso 1 1 calc R . . C8 C -0.4723(6) -0.0093(8) 0.2185(6) 0.0372(14) Uani 1 1 d . . . H8A H -0.5532 -0.0931 0.2215 0.056 Uiso 1 1 calc R . . H8B H -0.5309 0.0312 0.1561 0.056 Uiso 1 1 calc R . . H8C H -0.3980 0.0754 0.3201 0.056 Uiso 1 1 calc R . . C9 C 0.1258(7) -0.0133(6) 0.4196(5) 0.0261(10) Uani 1 1 d . . . H9A H 0.2124 0.0568 0.5228 0.039 Uiso 1 1 calc R . . H9B H 0.0393 -0.0959 0.4185 0.039 Uiso 1 1 calc R . . H9C H 0.0771 0.0465 0.3768 0.039 Uiso 1 1 calc R . . C10 C -0.0423(7) -0.4005(7) 0.2350(7) 0.0331(12) Uani 1 1 d . . . H10A H -0.1367 -0.5037 0.1828 0.050 Uiso 1 1 calc R . . H10B H -0.0534 -0.3303 0.3158 0.050 Uiso 1 1 calc R . . H10C H 0.0611 -0.4107 0.2769 0.050 Uiso 1 1 calc R . . C11 C -0.4123(7) -0.2348(6) 0.1164(7) 0.0399(14) Uani 1 1 d . . . H11A H -0.5032 -0.2810 0.1364 0.060 Uiso 1 1 calc R . . H11B H -0.3133 -0.2423 0.1761 0.060 Uiso 1 1 calc R . . H11C H -0.4449 -0.2914 0.0099 0.060 Uiso 1 1 calc R . . C50 C 0.2890(5) 0.3024(5) 0.3148(5) 0.0130(8) Uani 1 1 d . . . N1 N 0.1795(4) 0.1941(4) 0.2111(4) 0.0142(7) Uani 1 1 d . . . N2 N -0.3757(5) -0.0707(5) 0.1559(5) 0.0261(9) Uani 1 1 d . . . N3 N -0.0392(5) -0.3361(4) 0.1297(4) 0.0202(8) Uani 1 1 d . . . O1 O 0.0731(4) -0.1552(3) 0.0666(3) 0.0146(6) Uani 1 1 d . . . O2 O -0.1829(3) -0.0517(3) 0.0777(3) 0.0140(6) Uani 1 1 d . . . Cl1 Cl 0.63312(14) 0.49319(14) 0.35061(13) 0.0276(3) Uani 1 1 d . . . Cl2 Cl 0.59483(15) 0.33020(13) 0.57286(13) 0.0274(3) Uani 1 1 d . . . Fe1 Fe 0.0000 0.0000 0.0000 0.01394(19) Uani 1 2 d S . . Re1 Re 0.5000 0.5000 0.5000 0.01760(10) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.0140(19) 0.014(2) 0.018(2) 0.0067(17) 0.0089(17) 0.0091(17) C3 0.020(2) 0.021(2) 0.018(2) 0.0086(19) 0.0061(19) 0.0108(19) C4 0.0109(19) 0.021(2) 0.0108(19) 0.0035(17) 0.0005(17) 0.0040(17) C5 0.032(3) 0.017(2) 0.016(2) 0.0030(19) 0.009(2) 0.010(2) C6 0.031(3) 0.023(2) 0.017(2) 0.0086(19) 0.012(2) 0.018(2) C7 0.025(2) 0.019(2) 0.030(3) 0.009(2) 0.003(2) 0.000(2) C8 0.020(2) 0.063(4) 0.022(3) 0.009(3) 0.014(2) 0.016(3) C9 0.035(3) 0.030(3) 0.018(2) 0.011(2) 0.015(2) 0.019(2) C10 0.039(3) 0.034(3) 0.041(3) 0.029(3) 0.023(3) 0.014(2) C11 0.034(3) 0.027(3) 0.045(3) 0.007(3) 0.027(3) -0.005(2) C50 0.0112(19) 0.012(2) 0.013(2) 0.0042(18) 0.0049(18) 0.0042(18) N1 0.0142(18) 0.0142(18) 0.0112(18) 0.0041(16) 0.0054(16) 0.0044(16) N2 0.0175(19) 0.028(2) 0.022(2) -0.0003(18) 0.0140(17) 0.0034(17) N3 0.0196(19) 0.0189(19) 0.023(2) 0.0131(17) 0.0095(16) 0.0053(16) O1 0.0168(14) 0.0154(14) 0.0152(15) 0.0076(12) 0.0092(12) 0.0086(12) O2 0.0129(14) 0.0131(14) 0.0118(14) 0.0011(12) 0.0067(12) 0.0039(12) Cl1 0.0179(5) 0.0305(6) 0.0193(5) 0.0006(5) 0.0105(5) 0.0006(5) Cl2 0.0258(6) 0.0152(5) 0.0227(6) 0.0029(4) -0.0037(5) 0.0094(5) Fe1 0.0125(4) 0.0111(4) 0.0115(4) 0.0024(3) 0.0034(3) 0.0021(3) Re1 0.01417(14) 0.01391(14) 0.01421(14) 0.00136(10) 0.00254(10) 0.00294(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 O1 1.251(5) . ? C2 N3 1.335(6) . ? C2 C3 1.511(6) . ? C3 C9 1.526(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.242(6) . ? C4 N2 1.343(6) . ? C4 C6 1.515(6) . ? C5 C6 1.524(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N3 1.460(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N2 1.454(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N3 1.459(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N2 1.458(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C50 N1 1.147(6) . ? C50 Re1 2.116(4) . ? N1 Fe1 2.132(4) . ? O1 Fe1 2.084(3) . ? O2 Fe1 2.160(3) . ? Cl1 Re1 2.3291(11) . ? Cl2 Re1 2.3440(11) . ? Fe1 O1 2.084(3) 2 ? Fe1 N1 2.132(4) 2 ? Fe1 O2 2.160(3) 2 ? Re1 C50 2.116(4) 2_666 ? Re1 Cl1 2.3291(11) 2_666 ? Re1 Cl2 2.3440(11) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C2 N3 119.8(4) . . ? O1 C2 C3 119.5(4) . . ? N3 C2 C3 120.7(4) . . ? C2 C3 C9 111.9(4) . . ? C2 C3 H3A 109.2 . . ? C9 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C9 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O2 C4 N2 119.2(4) . . ? O2 C4 C6 121.3(4) . . ? N2 C4 C6 119.4(4) . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C5 111.8(4) . . ? C4 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C4 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C50 Re1 176.6(4) . . ? C50 N1 Fe1 170.5(3) . . ? C4 N2 C8 124.6(5) . . ? C4 N2 C11 118.7(4) . . ? C8 N2 C11 116.7(4) . . ? C2 N3 C10 124.3(4) . . ? C2 N3 C7 120.1(4) . . ? C10 N3 C7 115.6(4) . . ? C2 O1 Fe1 134.8(3) . . ? C4 O2 Fe1 139.5(3) . . ? O1 Fe1 O1 180.0(3) 2 . ? O1 Fe1 N1 88.41(13) 2 . ? O1 Fe1 N1 91.59(13) . . ? O1 Fe1 N1 91.59(13) 2 2 ? O1 Fe1 N1 88.41(13) . 2 ? N1 Fe1 N1 180.00(19) . 2 ? O1 Fe1 O2 86.54(11) 2 2 ? O1 Fe1 O2 93.46(11) . 2 ? N1 Fe1 O2 87.29(12) . 2 ? N1 Fe1 O2 92.71(12) 2 2 ? O1 Fe1 O2 93.46(11) 2 . ? O1 Fe1 O2 86.54(11) . . ? N1 Fe1 O2 92.71(12) . . ? N1 Fe1 O2 87.29(12) 2 . ? O2 Fe1 O2 180.00(19) 2 . ? C50 Re1 C50 180.0 2_666 . ? C50 Re1 Cl1 88.37(12) 2_666 2_666 ? C50 Re1 Cl1 91.63(11) . 2_666 ? C50 Re1 Cl1 91.63(12) 2_666 . ? C50 Re1 Cl1 88.37(11) . . ? Cl1 Re1 Cl1 180.0 2_666 . ? C50 Re1 Cl2 88.87(11) 2_666 2_666 ? C50 Re1 Cl2 91.13(11) . 2_666 ? Cl1 Re1 Cl2 90.57(5) 2_666 2_666 ? Cl1 Re1 Cl2 89.43(5) . 2_666 ? C50 Re1 Cl2 91.13(11) 2_666 . ? C50 Re1 Cl2 88.87(11) . . ? Cl1 Re1 Cl2 89.43(5) 2_666 . ? Cl1 Re1 Cl2 90.57(5) . . ? Cl2 Re1 Cl2 180.0 2_666 . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.879 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.139 #===END data_xwf23a _database_code_depnum_ccdc_archive 'CCDC 820657' #TrackingRef '- Structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common xwf23a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H52 Cl4 Fe N6 O4 Re' _chemical_formula_weight 896.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z' '-x, -y, -z' 'y-1/2, -x, -z' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z' _cell_length_a 13.3667(17) _cell_length_b 13.3667(17) _cell_length_c 10.7152(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1914.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9684 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 25.38 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 3.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8018 _exptl_absorpt_correction_T_max 0.8307 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 23640 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.40 _reflns_number_total 1770 _reflns_number_gt 1589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+5.9437P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1770 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.2500 0.2500 0.63915(3) 0.02159(13) Uani 1 4 d S . . Fe1 Fe 0.2500 0.2500 1.13743(10) 0.0173(2) Uani 1 4 d S . . Cl1 Cl 0.19880(8) 0.08241(8) 0.63692(10) 0.0296(3) Uani 1 1 d . . . O1 O 0.1344(2) 0.1418(2) 1.1401(3) 0.0283(7) Uani 1 1 d . . . C1 C 0.2500 0.2500 0.4426(7) 0.0203(16) Uani 1 4 d S . . C2 C 0.2500 0.2500 0.8359(8) 0.0257(18) Uani 1 4 d S . . C3 C 0.0991(4) 0.0755(4) 1.2118(5) 0.0433(12) Uani 1 1 d . . . C4 C 0.0337(5) 0.1053(5) 1.3231(6) 0.0539(15) Uani 1 1 d . . . H11A H 0.0355 0.1781 1.3335 0.081 Uiso 1 1 calc R . . H11B H 0.0592 0.0731 1.3989 0.081 Uiso 1 1 calc R . . H11C H -0.0353 0.0837 1.3081 0.081 Uiso 1 1 calc R . . C5 C 0.0746(4) -0.1021(4) 1.2605(7) 0.0545(16) Uani 1 1 d . . . H9A H 0.0619 -0.1574 1.2011 0.065 Uiso 1 1 calc R . . H9B H 0.0101 -0.0833 1.2992 0.065 Uiso 1 1 calc R . . C6 C 0.1477(6) -0.1381(6) 1.3629(8) 0.088(3) Uani 1 1 d . . . H10A H 0.2091 -0.1633 1.3239 0.133 Uiso 1 1 calc R . . H10B H 0.1163 -0.1918 1.4113 0.133 Uiso 1 1 calc R . . H10C H 0.1640 -0.0822 1.4184 0.133 Uiso 1 1 calc R . . C7 C 0.1832(4) -0.0464(5) 1.0858(6) 0.0545(15) Uani 1 1 d . . . H3A H 0.2383 0.0028 1.0803 0.065 Uiso 1 1 calc R . . H3B H 0.2130 -0.1130 1.1017 0.065 Uiso 1 1 calc R . . C8 C 0.1275(5) -0.0486(6) 0.9646(6) 0.074(2) Uani 1 1 d . . . H8A H 0.0692 -0.0926 0.9724 0.110 Uiso 1 1 calc R . . H8B H 0.1717 -0.0738 0.8987 0.110 Uiso 1 1 calc R . . H8C H 0.1053 0.0192 0.9435 0.110 Uiso 1 1 calc R . . N1 N 0.2500 0.2500 0.3356(6) 0.0249(15) Uani 1 4 d S . . N2 N 0.2500 0.2500 0.9438(7) 0.0293(16) Uani 1 4 d S . . N3 N 0.1142(3) -0.0184(3) 1.1947(4) 0.0422(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02652(15) 0.02652(15) 0.01174(18) 0.000 0.000 0.000 Fe1 0.0194(3) 0.0194(3) 0.0131(5) 0.000 0.000 0.000 Cl1 0.0322(6) 0.0264(5) 0.0302(6) 0.0019(4) -0.0014(4) -0.0021(4) O1 0.0298(16) 0.0258(16) 0.0294(16) 0.0060(13) -0.0004(13) -0.0064(12) C1 0.022(2) 0.022(2) 0.018(4) 0.000 0.000 0.000 C2 0.027(3) 0.027(3) 0.023(5) 0.000 0.000 0.000 C3 0.036(3) 0.046(3) 0.048(3) 0.003(2) -0.009(2) -0.005(2) C4 0.063(4) 0.053(3) 0.046(3) -0.003(3) -0.003(3) -0.012(3) C5 0.041(3) 0.033(3) 0.089(5) 0.014(3) 0.008(3) -0.006(2) C6 0.068(5) 0.063(5) 0.134(8) 0.056(5) -0.014(4) -0.013(4) C7 0.041(3) 0.050(3) 0.073(4) -0.015(3) 0.011(3) -0.005(2) C8 0.052(4) 0.112(6) 0.056(4) -0.011(4) 0.008(3) -0.007(4) N1 0.033(2) 0.033(2) 0.009(4) 0.000 0.000 0.000 N2 0.032(2) 0.032(2) 0.024(4) 0.000 0.000 0.000 N3 0.048(3) 0.030(2) 0.049(3) 0.0090(19) -0.012(2) -0.0134(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 2.106(8) . ? Re1 C2 2.108(8) . ? Re1 Cl1 2.3424(11) . ? Re1 Cl1 2.3424(11) 3 ? Re1 Cl1 2.3424(11) 4 ? Re1 Cl1 2.3424(11) 2 ? Fe1 N2 2.075(7) . ? Fe1 O1 2.117(3) 3 ? Fe1 O1 2.117(3) . ? Fe1 O1 2.117(3) 4 ? Fe1 O1 2.117(3) 2 ? Fe1 N1 2.124(7) 1_556 ? O1 C3 1.264(6) . ? C1 N1 1.147(11) . ? C2 N2 1.156(12) . ? C3 N3 1.285(7) . ? C3 C4 1.531(8) . ? C4 H11A 0.9800 . ? C4 H11B 0.9800 . ? C4 H11C 0.9800 . ? C5 N3 1.424(6) . ? C5 C6 1.546(9) . ? C5 H9A 0.9900 . ? C5 H9B 0.9900 . ? C6 H10A 0.9800 . ? C6 H10B 0.9800 . ? C6 H10C 0.9800 . ? C7 C8 1.497(9) . ? C7 N3 1.533(8) . ? C7 H3A 0.9900 . ? C7 H3B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N1 Fe1 2.124(7) 1_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C2 180.000(2) . . ? C1 Re1 Cl1 89.41(3) . . ? C2 Re1 Cl1 90.59(3) . . ? C1 Re1 Cl1 89.41(3) . 3 ? C2 Re1 Cl1 90.59(3) . 3 ? Cl1 Re1 Cl1 178.83(6) . 3 ? C1 Re1 Cl1 89.41(3) . 4 ? C2 Re1 Cl1 90.59(3) . 4 ? Cl1 Re1 Cl1 89.994(1) . 4 ? Cl1 Re1 Cl1 89.994(1) 3 4 ? C1 Re1 Cl1 89.41(3) . 2 ? C2 Re1 Cl1 90.59(3) . 2 ? Cl1 Re1 Cl1 89.994(1) . 2 ? Cl1 Re1 Cl1 89.994(1) 3 2 ? Cl1 Re1 Cl1 178.83(6) 4 2 ? N2 Fe1 O1 90.77(9) . 3 ? N2 Fe1 O1 90.77(9) . . ? O1 Fe1 O1 178.45(17) 3 . ? N2 Fe1 O1 90.77(8) . 4 ? O1 Fe1 O1 89.990(3) 3 4 ? O1 Fe1 O1 89.990(3) . 4 ? N2 Fe1 O1 90.77(8) . 2 ? O1 Fe1 O1 89.990(3) 3 2 ? O1 Fe1 O1 89.990(3) . 2 ? O1 Fe1 O1 178.45(17) 4 2 ? N2 Fe1 N1 180.000(3) . 1_556 ? O1 Fe1 N1 89.23(8) 3 1_556 ? O1 Fe1 N1 89.23(8) . 1_556 ? O1 Fe1 N1 89.23(8) 4 1_556 ? O1 Fe1 N1 89.23(8) 2 1_556 ? C3 O1 Fe1 139.4(3) . . ? N1 C1 Re1 180.000(1) . . ? N2 C2 Re1 180.000(2) . . ? O1 C3 N3 122.6(5) . . ? O1 C3 C4 120.3(5) . . ? N3 C3 C4 117.1(5) . . ? C3 C4 H11A 109.5 . . ? C3 C4 H11B 109.5 . . ? H11A C4 H11B 109.5 . . ? C3 C4 H11C 109.5 . . ? H11A C4 H11C 109.5 . . ? H11B C4 H11C 109.5 . . ? N3 C5 C6 111.2(5) . . ? N3 C5 H9A 109.4 . . ? C6 C5 H9A 109.4 . . ? N3 C5 H9B 109.4 . . ? C6 C5 H9B 109.4 . . ? H9A C5 H9B 108.0 . . ? C5 C6 H10A 109.5 . . ? C5 C6 H10B 109.5 . . ? H10A C6 H10B 109.5 . . ? C5 C6 H10C 109.5 . . ? H10A C6 H10C 109.5 . . ? H10B C6 H10C 109.5 . . ? C8 C7 N3 111.5(5) . . ? C8 C7 H3A 109.3 . . ? N3 C7 H3A 109.3 . . ? C8 C7 H3B 109.3 . . ? N3 C7 H3B 109.3 . . ? H3A C7 H3B 108.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 N1 Fe1 180.000(1) . 1_554 ? C2 N2 Fe1 180.000(2) . . ? C3 N3 C5 129.7(5) . . ? C3 N3 C7 116.2(5) . . ? C5 N3 C7 114.1(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.388 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.107 #===END